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Measurement of Palladium Crust Thickness on Catalysts by Optical Microscopy and Image Analysis

Published online by Cambridge University Press:  21 February 2013

Loïc Sorbier ,
Anne-Sophie Gay ,
Antoine Fécant ,
Maxime Moreaud  and
Nicolas Brodusch
Loïc Sorbier*
Affiliation:
IFP Energies nouvelles, Rond-point de l'échangeur de Solaize, P.O. Box 3, FR-69360 Solaize, France
Anne-Sophie Gay
Affiliation:
IFP Energies nouvelles, Rond-point de l'échangeur de Solaize, P.O. Box 3, FR-69360 Solaize, France
Antoine Fécant
Affiliation:
IFP Energies nouvelles, Rond-point de l'échangeur de Solaize, P.O. Box 3, FR-69360 Solaize, France
Maxime Moreaud
Affiliation:
IFP Energies nouvelles, Rond-point de l'échangeur de Solaize, P.O. Box 3, FR-69360 Solaize, France
Nicolas Brodusch
Affiliation:
McGill University, Mining and Materials Engineering Department, Wong Building, 3610 University Street, H3A 2B2 Montréal, Quebec, Canada
*
*Corresponding author. E-mail: loic.sorbier@ifpen.fr
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Abstract

Selective hydrogenation is an important process in petrochemistry to purify feedstock for polymer synthesis. For this process, catalysts containing metallic palladium deposited with an eggshell distribution on porous alumina are usually employed. For this kind of catalyst, the activity is known to be in close relation with the thickness of the palladium crust. As palladium oxide is brown and alumina is white, the palladium distribution in a catalyst bead before the reduction step can be characterized by optical microscopy. We propose an original and automatic procedure of optical image analysis to obtain a fast and robust method to measure the mean crust thickness of a catalyst batch and the corresponding standard deviation. The approach is validated by two different methods. First, we compared the crust thickness with those obtained by electron probe microanalysis. Then, catalytic tests of four samples with varying palladium crust thicknesses were performed and confirmed the expected correlation between activity and crust thickness measured by optical microscopy coupled with image analysis.

Keywords

image analysisoptical microscopyeggshell catalystselective hydrogenationEPMAcrust thickness
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 19 , Issue 2 , April 2013 , pp. 293 - 299
Copyright
Copyright © Microscopy Society of America 2013

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References

Berenblyum, A.S., Mund, S.L., Karel'skii, V.V., Goranskaya, T.P., Zolotukhin, V.E. & Lakhman, L.I. (1986). Catalysts for the selective hydrogenation of unsaturated compounds consisting of alumina particles with regular palladium distribution. Kinet Catal 27, 184–187.Google Scholar
Beucher, S. & Meyer, F. (1992). The morphological approach to segmentation: The watershed transformation. In Mathematical Morphology in Image Processing, Dougherty, E. (Ed.), pp. 433–481. New York: Marcel-Dekker.Google Scholar
Breen, E.J. & Jones, R. (1996). Attribute openings, thinnings and granulometries. Comp Vis Image Understand 64, 377–389.CrossRefGoogle Scholar
Brunauer, S., Emmet, P.H. & Teller, T. (1938). Adsorption of gases in multimolecular layers. J Am Chem Soc 60, 309–319.CrossRefGoogle Scholar
Chang, J.C. & Chou, T.C. (1997). Selective hydrogenation of isoprene over δ-alumina-supported eggshell Pd catalysts: Particle size effects. Appl Catal A 156, 193–205.CrossRefGoogle Scholar
Corbett, W.E. & Luss, D. (1974). The influence of non-uniform catalytic activity on the performance of a single spherical pellet. Chem Eng Sci 29, 1473–1483.CrossRefGoogle Scholar
Fischer, L., Petit-Clair, C., Thomazeau, C., Sorbier, L. & Verdon, C. (2007). Catalyst comprising palladium and selective hydrogenation application thereof. French Patent FR 2922784. Google Scholar
Iglesia, E., Soled, S.L., Baumgartner, J.E. & Reyes, S.C. (1995). Synthesis and catalytic properties of eggshell cobalt catalysts for the Fischer-Tropsch synthesis. J Catal 153, 108–122.CrossRefGoogle Scholar
Le Page, J.F. (1978). Catalyse de contact. Paris: Technip.Google Scholar
Lin, T.B. & Chou, T.C. (1994). Selective hydrogenation of isoprene on eggshell and uniform palladium profile catalysts. Appl Catal A 108, 7–19.CrossRefGoogle Scholar
Lin, T.B. & Chou, T.C. (1995). Pd migration. 1. A possible reason for the deactivation of pyrolysis gasoline partial hydrogenation catalysts. Ind Eng Chem Res 34, 128–134.CrossRefGoogle Scholar
Meyer, F. (1991). Method for the processing of images by hierarchically organized queues. French Patent FR 9103384. Google Scholar
Otsu, N. (1979). A threshold selection method from grey-level histograms. IEEE Trans Syst Man Cybern 9, 377–393.CrossRefGoogle Scholar
Salembier, P., Oliveras, A. & Garrido, L. (1998). Anti-extensive connected operators for image and sequence processing. IEEE T Image Proc 7, 555–570.CrossRefGoogle ScholarPubMed
Salembier, P. & Wilkinson, M.H.F. (2009). Connected operators: A review of region-based morphological image processing techniques. IEEE Signal Proc Mag 26(6), 136–157.CrossRefGoogle Scholar
Serra, J. (1988). Image Analysis and Mathematical Morphology—Vol. II. Theoretical Advances. London, UK: Academic Press.Google Scholar
Shadman-Yazdi, F. & Petersen, E.E. (1972). Changing catalyst performance by varying the distribution of active catalyst within porous supports. Chem Eng Sci 27, 227–237.CrossRefGoogle Scholar
Shao, Z., Li, C., Chen, X., Pang, M., Wang, X. & Liang, C. (2010). A facile and controlled route to prepare eggshell pd catalyst for selective hydrogenation of phenylacetylene. ChemCatChem 2, 1555–1558.CrossRefGoogle Scholar
Sorbier, L., Gay, A.-S., Fécant, A., Moreaud, M. & Brodusch, N. (2012). Measurement of palladium crust thickness on catalyst by EPMA. IOP Conf Ser Mater Sci Eng 32 012023. CrossRefGoogle Scholar
Sorbier, L., Rosenberg, E. & Merlet, C. (2004). Microanalysis of porous materials. Microsc Microanal 10, 745–752.CrossRefGoogle ScholarPubMed
Tomasi, C. & Manduchi, R. (1998). Bilateral filtering for gray and color images. Proc IEEEInt. Conf. Comput Vision, pp. 839–846.Google Scholar
Urbach, E.R. & Wilkinson, M.H.F. (2008). Efficient 2-D grayscale morphological transformations with arbitrary flat structuring elements. IEEE Trans Im Proc 17, 1–8.CrossRefGoogle ScholarPubMed
Villadsen, J. (1976). The effectiveness factor for an isothermal pellet with decreasing activity towards the pellet surface. Chem Eng Sci 31, 1212–1213.CrossRefGoogle Scholar
Vincent, L. (1993). Morphological grayscale reconstruction in image analysis: Applications and efficient algorithms. IEEE Trans Image Process 2, 176–201.CrossRefGoogle ScholarPubMed
Walter, T. (2003). Application de la morphologie mathématique au diagnostic de la rétinopathie diabétique à partir d'images couleur. Doctorate Thesis. Paris: Ecole des mines de Paris. Google Scholar